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Process for producing syndiotactic propylene polymer

a technology of syndiotactic propylene and polymer, which is applied in the direction of chemistry apparatus and processes, synthetic resin layered products, adhesive types, etc., can solve the problems of difficult to separate the copolymer, the molecular weight of the obtained copolymer is largely reduced, and the adhesion properties are inferior, etc., to achieve excellent adhesion properties, excellent thermal stability, and high graft ratio

Inactive Publication Date: 2010-02-25
MITSUI CHEM INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

The present invention provides a graft-modified syndiotactic propylene polymer with a high graft ratio and specific melt properties. The polymer is efficiently produced using a specific process. The resin composition containing the graft-modified polymer has good thermal stability and can be used as an adhesive agent in a laminate. The technical effects of the invention include improved adhesion and high-quality lamination.

Problems solved by technology

Although a copolymer of the syndiotactic polypropylene prepared in the above method or a propylene having a substantially syndiotactic structure and other olefins has relatively excellent physical properties, it has a problem such that since it is not compatible to other polymers having polar groups or metals, similar to isotactic polypropylenes, it is inferior in adhesion properties.
The preparation of the graft modified isotactic polypropylenes, however, has problems such that a obtained copolymer decreased largely in molecular weight by a simultaneous radical decomposition of polypropylene, which is a base polymer, or that it is difficult to separate the copolymer when it is prepared in a liquid phase.
The improvement, however, is necessary to be further improved in order to apply the polypropylene industrially because the graft efficiency is low, the syndiotactic polypropylene used herein has a racemic diad fraction [r] of from 0.51 to 0.88 and has low stereoregularity which is insufficient for improving the thermal stability, and further the production process of the dicarboxylic anhydride modified syndiotactic polypropylene is restricted to a solution method of using a radical initiator in the presence of a solvent.
However, the graft amount of the maleic anhydride used as a functional monomer is low, i.e. from 0.31% to 0.54%, and the great improvement in the capability as a binder with a polar resin cannot be found.

Method used

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  • Process for producing syndiotactic propylene polymer
  • Process for producing syndiotactic propylene polymer
  • Process for producing syndiotactic propylene polymer

Examples

Experimental program
Comparison scheme
Effect test

production example 1

[0167]To a 3 m3 internal volume reaction vessel thoroughly purged with nitrogen, 1000 liters of n-heptane was introduced and 610 ml (0.93 mol) of a toluene solution (Al=1.53 mol / L) of methylaluminoxane was added dropwise at ordinary temperature. To a 5 liters internal volume side-arm flask thoroughly purged with nitrogen, a magnetic stirrer was put. To the flask, 610 ml (0.93 mol) of a toluene solution (Al=1.53 mol / liter) of methylaluminoxane, and then 1.30 g (1.86 mmol) of a toluene solution of

dibenzylmethylene(cyclopentadienyl)(2,7-diphenyl-3,6-ditert-butylfluorenyl) zirconium dichloride were added, and stirred for 20 min. The resulting solution was added to the reaction vessel, and 3200 NL of hydrogen was fed at a rate of 19 Nm3 / h over 10 min. Thereafter, the polymerization was started while feeding 65 Kg / h of propylene. While the hydrogen gas phase concentration in the reaction vessel was kept to 53 mol % and propylene was continuously fed in an amount of 65 Kg / h, the polymeriza...

example 1

[0168]100 parts by weight of the syndiotactic polypropylene prepared in Production Example 1 was dry blended with a solution prepared by dissolving 1.5 parts by weight of maleic anhydride (abbreviated to MAH, manufactured by Wako Pure Chemical Industries Ltd.), 1.5 parts by weight of t-butyl peroxy benzoate (Trade Name Perbutyl Z, manufactured by NOF Corporation) in acetone. Thereafter, melt modification was carried out using a twin axial kneader (KZW15, manufactured by Technovel Corporation) at a resin temperature of 180° C., at a screw rotation number of 200 rpm, and at an output rate of 25 g / min. In the extrusion, a radical initiator, a solvent, and unreacted maleic anhydride were deaerated in vacuo. After cooling, an extruded strand in a molten state was pelletized to prepare maleic acid-modified syndiotactic polypropylene (hereinafter abbreviated to MAH-sPP-1) having an rrrr fraction of 0.92, a graft amount of 1.30% by weight and MFR of 91 g / 10 min. The MAH-sPP had an internal ...

example 2

[0169]The procedure of the melt modification of Example 1 was repeated except for using 1.5 parts by weight of maleic anhydride and 1.5 parts by weight of t-butyl peroxy benzoate, and changing the resin temperature to 230° C. After cooling, an extruded strand in a molten state was pelletized to prepare maleic acid-modified syndiotactic polypropylene (hereinafter abbreviated to MAH-sPP-2) having a graft amount of 1.43% by weight and MFR of 392 g / 10 min. The results are shown in Table 1.

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Abstract

Disclosed is a graft-modified syndiotactic propylene polymer having a high graft ratio. Also disclosed are a method for producing such a polymer, a resin composition containing such a polymer, and a laminate having at least one layer which contains the composition as an adhesive resin composition. Specifically disclosed is a graft-modified syndiotactic propylene polymer which is characterized by satisfying the following characteristics [1]-[3]. [1] The melt flow rate (MFR) measured at 230° C. under a load of 2.16 kg is 30-1000 (g / 10 minutes). [2] The concentration of graft groups derived from a radically polymerizable unsaturated compound by 1H-NMR measurement is within the range of 0.7-7.0% by weight. [3] The syndiotactic pentad fraction determined by 13C-NMR measurement is not less than 0.80.

Description

TECHNICAL FIELD OF THE INVENTION[0001]The present invention relates to a graft modified syndiotactic propylene polymer, a process for producing the polymer, a thermoplastic resin composition containing the polymer and their uses. Specifically, it relates to a propylene copolymer obtainable by graft polymerizing a radical polymerizing unsaturated compound on a syndiotactic propylene homopolymer having a relatively high tacticity or a copolymer of propylene and a small amount of other olefins, and a process for producing the copolymer, and it also relates to their uses.BACKGROUND OF THE INVENTION[0002]As isotactic polypropylenes are low in price and have a relatively good balance in physical properties, they have various uses. Meanwhile, the existence of syndiotactic polypropylenes has been known. However, a known method of polymerizing at a low temperature in the presence of a catalyst comprising a vanadium compound, ether and an organoaluminum has low levels of syndiotacticity and i...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): C08L33/02
CPCB32B7/12B32B27/32C08F255/02C08L51/06C09J151/06C08L2666/04C08L2666/02
Inventor SOEDA, YASUYUKIONOGI, TAKAYUKIMORIOKAMOTO, MASAHIKOKAGEYAMA, FUMIO
Owner MITSUI CHEM INC
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